Process of producing titanium cyanonitrids.



is more fully hereinafter SAMUEL PEACOCK, OF CHICAGO,

POWDER COMPANY;

rumors,

A coaromrron or new masmr.

.nssronoa To a. 1. no ron'r m: nnnoons PROCESS OF PRODUCING TI'IANIUE CYANONITB-IDS.

1,088,359. No Drawing.

Specification of Letters Patent. Application filed November M, 1911. Serial No. 882,280.

Patented Feb. 24, 1914.

To all whom it may concern Be it known that I, SAMUEL Pnnooox a citizen of the United States, residing at C icago, in the county of Cook and State of Illmois, have invented certain new and useful Improvements in Processes of Producing Titanium Cyanonitrids; and I do hereby def clare the following'to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

This invention relates to the production of titanium cyanoenitrids of which there are two forms of commercial importance, viz:

1 TiO,N, 2 TiCN,

and has for its object to provide a process for making these products in an eflicient and expeditious manner.

. To these ends the invention consists in the novel steps constituting my invention,-which disclosed, and particularly pointed out in the claims.

Any suitable form of furnace, not shown, may be employed in carrying out my process, one instance being that illustrated in my 00- pending application No. 650,973, filed September 23, 1911, for process of producing compounds of aluminum, carbon and nitrogen.

More particularly stated, this process consists in taking advantage of the relation which exists between the equilibrium temperatures and pressures of the formation of titanium carbids and nitrogen containing titanium compounds, the exact nature of which I have not as yet determined, but which I believe to be and will titanium cyano-nitrids to form them at a temperature in the neighborhood of 1800 C-., and at a total pressure of about two atmospheres or higher, while the partial pressure of carbon monoxid CO in the furnace is below that of the atmosphere, or say at 100 to 200 millimeters of mercury, or lower.

In carrying out my process, I take finely divided and dry titanium oxid Ti(),, and finely divided and dry carbon, preferably as coke or charcoal, and mix the same together thoroughly, in chemically equivalent procall herein portions conforming to the following equat1ons:--

v I may, however, and preferably use carbon in excess of that necessary for the above.

reaction, to the extent of 20 to 30 per cent,

' more or less, in order to prevent the formation of titanium nitrids, which contain a lower percentage of nitrogen than do my titanium cyano-nitrids. Further, said excess of carbon insures the more ready complete conversion of the titanium to the cyano-nitrid form, to the process.

I am aware that the carbid of titanium commonly known, consists of one equivalent each of titanium and carbon (TiC), and such is the form of carbid usually obtained when treating a mixture of titanium and carbon at temperatures of 1800 C. and higher under atmospheric pressure, and also in the presence of carbon monoxid CO the product of the reaction at a partial pressure of about one-half an atmosphere or higher. But under such conditions of a comparatively high partial pressure, unless the mass is molten and the total pressure on the mixture vastly increased, the higher carbids cannot exist because they will be dissociated as fast as formed to the lower car bids. For example, calcium carbid CaC when heated at about 1000 C.'to 1200 C. in a vacuum or in an atmosphere of inert gas, breaks down from GaC to CaO. In other words, as is well known, under suitable conditions, although higher metallic carbids of the acetylene forminggroup such as GaC or TiC,, and of the ethylene forming group such as ,CaC, or TiC,, may they will beimmediately dissociated into a methane forming group such as Ca,C or TiC, unless the pressure is maintained at a high point, and the temperature correspondingly raised. Of course, however, should the temperature be lowered in such case, the

oxid

be formed, yet

tem erature higher than 1800 mi pressure is employed, and pressure .of carbon monoxid not exceeding 20 per cent. or less of the'said total presthe furnace of two atmospheres rapidly unless sure. -An example illustrating these conditions is given as follows :'C alcium carbid CaC, isreadil formed, when a mixture of calcium'oxid JaO and carbon-"is heated to such temperatures that the lime becomes uite fluid and a molten mass is formed.

uch temperatures will be as high as from say 2500 O. to3000 0. Under these hydrostatic conditions, the pressure in the mass rises above that of the atmosphere 760 m.- m., while the molten charge isv comparatively low in carbon monoxid CO, and therefore while the partial pressure of the latter is less than 760 m. m. By my process, therefore, it will be seen that I may produce these higher carbids at a tem rature' of about 1800 C. by maintaining fife partial pressure of the carbon monoxid as low as from 100 to 200 m. m. and by employing a total pressure in about two atmospheres or however, the main object of the production of titanium preferably maintain these of pressure by the controlled admission of nitrogen into the furnace, while carbon monoxid is being liberated as a result of the following reaction The velocity of this reaction decreases the temperature is raised, but mcreasing the temperature tends to dissociate the higher carbid to the lower form higher. Since, my process is cyano-nitrid, I

. TiQ, wh1ch is undesirable, Therefore, I

7 the reaction (a) 60.

maintain a steady flow at a constant pressure of nitrogen over the heated mixture; the carbon monoxid being thus removed by the escape of nitrogen as rapidly as it is formed. In this manner, I maintain a very low carbon monoxid partial ressure to facilitate the formation of the igher carbids while the nitrogen reacts with the latter to form the. cyano-nitrids, in accordance with the following equations Both reactions occur simultaneously, but proceeds under lower tem-. peratures and much lower carbon monoxid partial pressures than does, reaction (6).

the mechanical limitations. of the furnace do notenable me to maintain a constant absence of carbon monoxid from the if a higher also a partial? 'tanium' oxid The. industrial advantage of producing tlt'anium cyano-nitrid over prodncingtitw nium nitrid Ti N is that the former efiects the fixation of more nitrogen per unit of metallic oxid than the latter, and also at a lower consumption of energy; also, the titanium cyano nitrid is capable of conversion into organic nitrogen compounds of high industrial value, whereas the nitrid Ti ,N may be efiectively converted into ammonia only.

Itis obvious that those skilled in the art may vary the details of my process without departingfrom the spirit thereof,3and therefore I do not wish to be-limited to the above disclosure except as may be required by the claims.

What I claim is:

1. The process of producing nitrogen containing titanium compounds which consists in heating, in the presence of nitrogen, timixed with carbon to a temperature sutlicient to produce said compounds while maintaining the partial pres sure of the evolved carbon monoxid not substantially higher than 200 millimeters of mercury, substantially as described.

2. The processcof taining titanium compounds which consists in heating, in the presence of nitrogen, titanium oxid mixed with carbon under a total pressure not substantially less than two atmospheres and to a temperature suflicient to produce said compounds while maintaining the partial pressure of the evolved carbon monoxid not substantially higher than 200 millimeters of mercury, substantially as described' 3. The process of producing nitrogen containing titanium compoundswhich consists in heating, in the presence of nitrogen, under a pressure not substantially less than two atmospheres, a mixture of titanium oxid and carbon at a temperature of substantially 1800 C. to produce said compounds while maintaining the partial pressure of the evolved carbon monoxid not substantially higher than 200 eters of mercury, substantiall as described.

4. The process 0 producing nitrogen containing titanium compounds which consists in heating, 1n the resence of nitro en, under a pressure not su stantially less t an two atmospheres, 'a mixture of titanium oxid and carbon the latter being in excess of that required for a chemically equivalent proport1on and at a temperature of substantially 1800 C. to produce said compounds while maintaining the partial pressure of the producing nitrogen conevolved carbon monoxid not substantially higher than 200 millimeters of mercury, substantially as described.

5. The process of producing the higher carbids of titanium which consists in heating a mixture of titanium oxid and carbon to a temperature sufficient to produce said carbids while maintaining the partial pressure of the evolved carbon monoxid not substantially higher than 200 millimeters of 10 mercury, substantially as described.

In testimony whereof, I afiix my signature, in presence of two witnesses.

SAMUEL PEAGOCK.

Witnesses:

T. A. Wrrrmnsroon, GEO. B. Prrrs. 

